CN104193340B - Doctor-blade casting process is for the preparation of the method for the AlN ceramic chips of multi-layer wire substrate and obtained AlN ceramic chips - Google Patents
Doctor-blade casting process is for the preparation of the method for the AlN ceramic chips of multi-layer wire substrate and obtained AlN ceramic chips Download PDFInfo
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Abstract
The invention discloses the method for a kind of doctor-blade casting process for the preparation of the AlN ceramic chips of multi-layer wire substrate, comprise AlN multilayer ceramic chips, slurry making method and casting technique, that AlN powder, sintering aid, dispersion agent, binding agent, softening agent and stirring solvent are mixed, form slurry, ceramic chips is obtained again by the method for curtain coating, ceramic chips gauge control is at below 0.300mm, and made ceramic chips can meet multi-layer wire substrate and make requirement.
Description
Technical field
The present invention relates to novel photoelectric communication Material Field, be one of key areas of electronic ceramics encapsulation technology development, be specifically related to a kind of AlN ceramic chips for photoelectric communication industry and curtain coating preparation method thereof.
Background technology
The multifunction of the equipment such as electronic information, power electronics, semiconductor laser, photovoltaic industry and the raising day by day of the level of automation characteristics such as function is complete, volume is little, quality is light, high-level efficiency, high power density that require electronics systems to have, thus facilitate relevant electron device to develop rapidly towards high-power, highly integrated and microminiaturized direction, a lot of product needed at substrate indoor design multi-layer precise circuit, thus reaches electron device demand.Meanwhile, higher requirement be it is also proposed to the quality of electronic circuit bearing substrate supporting with it, especially at thermostability and thermal conductivity aspect of performance.Traditional ceramic bearing substrate mainly contains Al
2o
3, BeO.Wherein, Al
2o
3the thermal conductivity (20-30W/ (mK)) of substrate is low, and heat dispersion does not reach requirement; BeO is eliminated gradually because of expensive and hypertoxic.So that the high heat conductance of 160-230W/ (mK), low-k, thermal stability be good etc., advantage replaces traditional Al to AlN gradually
2o
3, BeO substrate.At present, AlN substrate shows huge superiority in fields such as high power module circuit, semiconductor laser and LED, has the extensive market space.
The common forming method of AlN substrate has dry-pressing formed, injection moulding and flow casting molding (tapecasting) etc., wherein substrate that is dry-pressing formed, injection moulding can not meet inner multilayer wiring requirement, and the ceramic chips only having casting molding processes to make could meet the requirement of its inner multilayer wiring.In addition, it is high that doctor-blade casting process also has production efficiency, the repeatability of molding blank and dimensional uniformity high, and being suitable for big area, various shape substrate and encapsulating products and making, is the desirable forming method of multilayer ceramic ceramic chips.Casting molding processes is divided into water base and non-water based system two kinds, and the patent of invention of aqueous based systems casting technology has: the aqueous tape casting method of patent 200910049377.5 (publication number 101863071A) a kind of superhigh temperature ceramics and patent 200410016144.2 (publication number 11557776) water base casting process make the method for high-heat conductivity aluminium nitride ceramics substrate.There is AlN powder and must carry out long, the drying of resistant to hydrolysis process, slurry drying time and easily occur the deficiencies such as tiny crack in this technique.Current water-based tape casting technology is also in the laboratory study stage, not for large-scale production.The patent of invention of non-water based system casting technology has: patent 200810224311.0 (publication number 101386539) aluminium nitride ceramics material and preparation method thereof, the making method of patent 200810142697.0 (publication number 101333114) a kind of high-thermal-conductivity aluminium nitride ceramics substrate and patent 03100287.0 (publication number 1421418) high-heat conductivity aluminium nitride ceramics etc.The curtain coating ceramic chips thickness of this explained hereafter is generally more than 0.3mm, and the ceramic chips obtained is mainly used to make photopolymer substrate (inside is containing metal circuit not), and is not suitable for multilager base plate (indoor design metal line) and makes demand.
The AlN multilager base plate of photoelectric communication industry generally needs to prepare ceramic chips by casting method, then multilager base plate is being processed as through postchannel process, shown in specific as follows: AlN multilager base plate making processes adopts casting technology to make the ceramic chips (below thickness 0.3mm) being applicable to multilayer, and then by beginning to speak to ceramic chips punching, the technique such as filling through hole slurry (tungsten slurry etc.), conduction band printed wiring (tungsten slurry etc.), lamination is made for certain thickness laminated ceramic chips, then is made for multilayer AlN ceramic by the technique such as binder removal, sintering.Current AlN multilayer wiring Technology can reach more than 30 layers at most, meet the wiring requirement that electron device develops rapidly towards high-power, highly integrated and microminiaturized direction, but this technology is very high to the specification of quality of ceramic chips, such as: 1) ceramic chips will have certain intensity and snappiness, be easy to punching and begin to speak; 2) contraction of ceramic chips is mated with the contraction phase of Metal slurry; 3) organism such as the binding agent added in technological process easily under inertia or reducing atmosphere low-temperature decomposition drain; 4) the thickness general control of ceramic chips is 0.05 ~ 0.300mm; 5) ceramic chips caliper uniformity is good, and thickness deviation controllability is good.
Summary of the invention
The object of the present invention is to provide a kind of doctor-blade casting process for the preparation of the method for the AlN ceramic chips of multi-layer wire substrate and the AlN ceramic chips prepared, made ceramic chips can meet photoelectric communication industry multi-layer wire substrate and make demand.
Technical scheme of the present invention is as follows:
A kind of doctor-blade casting process is for the preparation of the method for the AlN ceramic chips of multi-layer wire substrate, it is characterized in that: AlN powder, sintering aid, dispersion agent, binding agent, softening agent and stirring solvent are mixed, form slurry, ceramic chips is obtained again by the method for curtain coating, ceramic chips gauge control is at below 0.300mm, and concrete making step is as follows:
1) sintering aid, dispersion agent and curtain coating are added solvent and carry out first time ball milling;
2) AlN powder is added in first time ball milling system, then carry out second time ball milling;
3) after above-mentioned ball milling, add binding agent and softening agent in mixed system, carry out third time ball milling;
4) after third time, ball milling terminated, slurry is transferred to system in vacuum defoamation system and carry out deaeration;
5) deaeration disposed slurry is carried out curtain coating, obtain casting films;
6) casting films is carried out drying under drying system, obtain curtain coating ceramic chips;
7) by cutting inspection, the ceramic chips of desired size is obtained.
Described doctor-blade casting process, for the preparation of the method for the AlN ceramic chips of multi-layer wire substrate, is characterized in that, specifically comprises the following steps:
1) load weighted sintering aid and dispersion agent are joined in the multicomponent solvent mixed and carry out first time ball milling, the rotating speed of ball milling is 30 ~ 60r/min, and the time is 20 ~ 150min;
2) load weighted AlN powder is joined above-mentioned 1) in mixed solution after ball milling, carry out second time ball milling; The rotating speed of ball milling is 50 ~ 80r/min, and the time is 60 ~ 300min;
3) above-mentioned 2) add binding agent and softening agent respectively in powder mixed solution after ball milling, be uniformly mixed and carry out third time ball milling, the rotating speed of ball milling is 50 ~ 80r/min, and the time is 600 ~ 1200min;
4) 3 are tested) viscosity of step ball milling disposed slurry, after ball milling, viscosity controller is at 1000 ~ 6000mPa.s, then slurry is transferred in vacuum defoamation system and carry out deaeration, vacuum degree control-25PSI, stir speed (S.S.) is 30 ~ 120r/min, inclined heated plate 30 ~ 400min, after deaeration, viscosity controller is at 2000 ~ 10000mPa.s;
5) deaeration disposed slurry being pressurized in curtain coating groove, by adjustment curtain coating scraper gap than controlling curtain coating ceramic chips thickness, thus obtaining different thickness casting films;
6) casting films is carried out drying in different warm area, control intensification drying rate by the mode of upper heating, lower heating and wind-heat.In order to obtain stable performance and the measured ceramic chips of matter, preferred drying system is to cool mode in heat up in stage heating and stage, mainly prevents ceramic chips from causing the defects such as the cracking of ceramic chips, tiny crack and warpage because liter (falling) speed is too fast.Warm area arranges drying system: the first warm area temperature is 25 ~ 45 DEG C, second warm area temperature is 40 ~ 60 DEG C, and three-temperature-zone temperature is 55 ~ 70 DEG C, and four-temperature region temperature is 60 ~ 100 DEG C, 5th warm area temperature is 45 ~ 70 DEG C, and the 6th warm area temperature is 25 ~ 50 DEG C.
Described doctor-blade casting process, for the preparation of the method for the AlN ceramic chips of multi-layer wire substrate, is characterized in that:
Described AlN powder requires that mean particle size is between 0.8 ~ 2.5 μm, and specific surface area is 2 ~ 4.5 ㎡/g, and oxygen level is less than 0.9%;
Described sintering aid is one or both in rare-earth oxide, alkaline earth metal oxide Y2O3, CaO, MgO;
Described dispersion agent be oleic acid, triolein, fish oil, acrylic resin etc. one or both;
Described binding agent is polymerized thylene carbonate third fat resin;
Described softening agent be dimethyl phthalate (DMP) and butyl benzyl phthalate (BBP) one or both;
Described solvent is the Diversity system in Virahol, acetone, butanone, ethanol.
Described doctor-blade casting process, for the preparation of the method for the AlN ceramic chips of multi-layer wire substrate, is characterized in that:
The mass ratio of described AlN powder, sintering aid, dispersion agent, binding agent, softening agent, solvent can carry out proportioning according to casting thickness.
Described doctor-blade casting process, for the preparation of the method for the AlN ceramic chips of multi-layer wire substrate, is characterized in that:
The mass ratio of described AlN powder, sintering aid, dispersion agent, binding agent, softening agent, solvent is 1:0.03 ~ 0.07:0.01 ~ 0.03:0.05 ~ 0.30:0.03 ~ 0.05:0.70 ~ 0.90.
AlN ceramic chips for photoelectric communication industry prepared by present method.
The present invention compared with prior art tool has the following advantages:
1. the present invention adopts the multicomponent solvent systems such as acetone, butanone, Virahol, can prevent solvent in slurry from volatilizing in short-term in a certain warm area, thus affect the internal soundness of ceramic chips; Multicomponent solvent instead of traditional benzene, toluene is main solvent system, reduces toxic gas discharge, reduces environmental pollution, reduce production cost.
2. the present invention uses polymerized thylene carbonate third fat resin glue to replace polyvinyl butyral acetal (PVB), easily should decompose at inert atmosphere, and decomposition temperature low (less than 450 DEG C), degradation production is carbonic acid gas and water, in laminated ceramic chips after binder removal, carbon foreign matter content is low, is conducive to the performance improving multilager base plate, overcomes conventional binders and decompose not thorough under this atmosphere, carbon residual quantity is high, affects substrate performance;
3. the present invention takes three ball milleds, ensure sintering aid, powder, dispersion agent, binding agent, softening agent be uniformly dispersed, the consistence of slurry is good, in this technological process balls grinding media and ball grinder material wear resistance good, abrasion loss is low, the strict introducing controlling impurity;
4. dry heat of the present invention takes heating, lower heating and wind-heat three kinds of modes to heat, thus ensure that ceramic chips is heated evenly up and down, and the solvent of ceramic chips volatilization can be taken away in time; Meanwhile, take segmentation falling temperature method, decrease the disadvantageous effect of temperature decrease to ceramic chips performance, reduce the warpage at ceramic chips edge;
5. the ceramic chips intensity of the present invention's production is high, snappiness good, surface smoothness good, caliper uniformity is good, can meet the requirement of the multilayered printed lamination of AlN well, simultaneously, ceramic chips product thickness of the present invention, at 0.100mm ~ 0.300mm, meets the ceramic chips printed wiring of 30 layer multi-layer substrates, the processing requirements such as punches and begin to speak.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of doctor-blade casting process of the present invention for the preparation of the method for the AlN ceramic chips of multi-layer wire substrate.
Embodiment
Embodiment one
Curtain coating 0.100mm improves people's living condition ceramics
The mean particle size of AlN powder is 1.2 μm, and specific surface area (BET) is 3.4 ㎡/g, oxygen level < 0.9% (weight percent), Y
2o
3, CaO diameter of particle is all within the scope of 0.8 ~ 3.0 μm.
This example is prepared burden according to following proportioning:
AlN powder weight percent is 47%
Sintering aid weight percent is 2.5%
Dispersant weight per-cent is 0.95%
Weight of binder per-cent is 8.5%
Multicomponent solvent weight percent is 37.3%
Softening agent per-cent is 3.75%
1) prepare 3.5kg batch and carry out curtain coating.Dispersion agent, sintering aid and multicomponent solvent is weighed according to aforementioned proportion.Pour into after solvent in ball grinder, then sintering aid and dispersion agent are joined in multicomponent solvent respectively stir.Carry out first time ball milling after mixing, the rotating speed of ball milling is 40r/min, and the time is 120min;
2) load weighted AlN powder is joined above-mentioned 1) in mixed solution after ball milling, carry out second time ball milling; The rotating speed of ball milling is 70r/min, and the time is 240min;
3) above-mentioned 2) add binding agent and softening agent respectively in powder mixed solution after ball milling, be uniformly mixed and carry out third time ball milling, the rotating speed of ball milling is 60r/min, and the time is 960min;
4) ball milling terminates rear test 3) viscosity of step ball milling disposed slurry, after ball milling, viscosity is 1800mPa.s (T=303K); Then slurries filtration is transferred in vacuum defoamation system and carry out deaeration; Vacuum degree control is at-20PSI, and stir speed (S.S.) is 60r/min, inclined heated plate 20min, and after deaeration, viscosity controller is at 2260mPa.s;
5) be pressurized in curtain coating groove by deaeration disposed slurry, curtain coating scraper gap is 0.37mm;
6) heating, lower heating and wind-heat warm area temperature are set, and curtain coating belt speed and liquid level.Design parameter is arranged as table 1
| Initial viscosity | Deaeration viscosity | Inclined heated plate | Marly thickness | Belt speed | Liquid level | Scraper gap |
| 1800mPa.s | 2260mPa.s | 20min | 75μm | 40cm/min | 20cm | 0.37mm |
| Warm area | Zone 1 | Zone 2 | Zone 3 | Zone 4 | Zone 5 | Zone 6 |
| Wind-heat | 30 | 40 | 55 | 60 | 50 | 30 |
| Upper heating | 40 | 50 | 60 | 75 | 60 | 40 |
| Lower heating | 40 | 55 | 70 | 80 | 60 | 40 |
Curtain coating green band draws through cutting inspection:
Mean thickness: 0.104mm;
Thickness deviation :≤± 5%;
Ceramic chips density: 2.07g/cm
3;
X, Y-direction contraction ratio: 1.192;
Z-direction contraction ratio: 1.213;
Embodiment two
Curtain coating 0.168mm improves people's living condition ceramics
The mean particle size of AlN powder is 1.2 μm, and specific surface area (BET) is 3.4 ㎡/g, oxygen level < 0.9% (weight percent), Y
2o
3, CaO diameter of particle is all within the scope of 0.8 ~ 3.0 μm.
This example is prepared burden according to following proportioning:
AlN powder weight percent is 47%
Sintering aid weight percent is 2.5%
Dispersant weight per-cent is 0.95%
Weight of binder per-cent is 8.5%
Multicomponent solvent weight percent is 37.3%
Softening agent per-cent is 3.75%
1) prepare 3.5kg batch and carry out curtain coating.Dispersion agent, sintering aid and multicomponent solvent is weighed according to aforementioned proportion.Pour into after solvent in ball grinder, then sintering aid and dispersion agent are joined in multicomponent solvent respectively and stir, carry out first time ball milling after mixing, the rotating speed of ball milling is 40r/min, and the time is 120min;
2) load weighted AlN powder being joined above-mentioned 1) in mixed solution after ball milling, carry out second time ball milling, the rotating speed of ball milling is 70r/min, and the time is 240min;
3) above-mentioned 2) add binding agent and softening agent respectively in powder mixed solution after ball milling, be uniformly mixed and carry out third time ball milling, the rotating speed of ball milling is 60r/min, and the time is 960min;
4) ball milling terminates rear test 3) viscosity of step slurry, after ball milling, viscosity is 2320mPa.s (T=303K), is then transferred in vacuum defoamation system by slurries filtration and carries out deaeration; Vacuum degree control is at-20PSI, and stir speed (S.S.) is 60r/min, inclined heated plate 30min, and after deaeration, viscosity controller is at 2850mPa.s;
5) be pressurized in curtain coating groove by deaeration disposed slurry, curtain coating scraper gap is 0.55mm;
6) heating, lower heating and wind-heat warm area temperature are set, and curtain coating belt speed and liquid level.Design parameter is arranged as table 2
| Initial viscosity | Deaeration viscosity | Inclined heated plate | Marly thickness | Belt speed | Liquid level | Scraper gap |
| 2320mPa.s | 2850mPa.s | 30min | 75μm | 40cm/min | 20cm | 0.55mm |
| Warm area | Zone 1 | Zone 2 | Zone 3 | Zone 4 | Zone 5 | Zone 6 |
| Wind-heat | 30 | 45 | 60 | 60 | 50 | 30 |
| Upper heating | 40 | 55 | 60 | 75 | 60 | 40 |
| Lower heating | 40 | 60 | 70 | 85 | 60 | 40 |
Curtain coating green band draws through cutting inspection:
Mean thickness: 0.162mm;
Thickness deviation :≤± 5%;
Ceramic chips density: 2.05g/cm
3;
X, Y-direction contraction ratio: 1.198;
Z-direction contraction ratio: 1.215;
Embodiment three
Curtain coating 0.270mm improves people's living condition ceramics
The mean particle size of AlN powder is 1.2 μm, and specific surface area (BET) is 3.4 ㎡/g, oxygen level < 0.9% (weight percent), Y
2o
3, CaO diameter of particle is all within the scope of 0.8 ~ 3.0 μm.
This example is prepared burden according to following proportioning:
AlN powder weight percent is 48.3%
Sintering aid weight percent is 2.58%
Dispersion agent per-cent is 0.97%
Binding agent per-cent is 5.8%
Multicomponent solvent weight percent is 38.4%
Softening agent per-cent is 3.95%
1) prepare 7kg batch and carry out curtain coating.Dispersion agent, sintering aid and multicomponent solvent is weighed according to aforementioned proportion.Pour into after solvent in ball grinder, then sintering aid and dispersion agent are joined in multicomponent solvent respectively stir.Carry out first time ball milling after mixing, the rotating speed of ball milling is 40r/min, and the time is 120min;
2) load weighted AlN powder being joined above-mentioned 1) in mixed solution after ball milling, carry out second time ball milling, the rotating speed of ball milling is 70r/min, and the time is 240min;
3) above-mentioned 2) add binding agent and softening agent respectively in powder mixed solution after ball milling, be uniformly mixed and carry out third time ball milling, the rotating speed of ball milling is 60r/min, and the time is 960min;
4) ball milling terminates rear test 3) viscosity of step slurry, after ball milling, viscosity is 1250mPa.s (T=303K), then slurries filtration is transferred to vacuum defoamation system and carry out deaeration, vacuum degree control is at-25PSI, stir speed (S.S.) is 60r/min, inclined heated plate 90min, after deaeration, viscosity general control is at 4850mPa.s;
5) be pressurized in curtain coating groove by deaeration disposed slurry, curtain coating scraper gap is 0.740mm;
6) heating, lower heating and wind-heat warm area temperature are set, and curtain coating belt speed and liquid level.Design parameter is arranged as table 3
| Initial viscosity | Deaeration viscosity | Inclined heated plate | Marly thickness | Belt speed | Liquid level | Scraper gap |
| 1250mPa.s | 4850mPa.s | 90min | 125μm | 25cm/min | 30cm | 0.74mm |
| Warm area | Zone 1 | Zone 2 | Zone 3 | Zone 4 | Zone 5 | Zone 6 |
| Wind-heat | 30 | 40 | 55 | 60 | 50 | 30 |
| Upper heating | 40 | 50 | 65 | 75 | 70 | 40 |
| Lower heating | 40 | 55 | 75 | 85 | 70 | 40 |
The dry green band out of curtain coating draws through cutting inspection:
Mean thickness: 0.274mm;
Thickness deviation :≤± 5%;
Ceramic chips density: 2.10g/cm
3;
X, Y-direction contraction ratio: 1.203;
Z-direction contraction ratio: 1.218.
Claims (5)
1. a doctor-blade casting process is for the preparation of the method for the AlN ceramic chips of multi-layer wire substrate, it is characterized in that: AlN powder, sintering aid, dispersion agent, binding agent, softening agent and stirring solvent are mixed, form slurry, ceramic chips is obtained again by the method for curtain coating, ceramic chips gauge control is at below 0.300mm, described binding agent is polymerized thylene carbonate third fat resin, and described solvent is the Diversity system in Virahol, acetone, butanone, ethanol;
Its making step is as follows:
1) load weighted sintering aid and dispersion agent are joined in the multicomponent solvent mixed and carry out first time ball milling, the rotating speed of ball milling is 30 ~ 60r/min, and the time is 20 ~ 150min;
2) load weighted AlN powder is joined above-mentioned 1) in mixed solution after ball milling, carry out second time ball milling; The rotating speed of ball milling is 50 ~ 80r/min, and the time is 60 ~ 300min;
3) above-mentioned 2) add binding agent and softening agent respectively in powder mixed solution after ball milling, be uniformly mixed and carry out third time ball milling, the rotating speed of ball milling is 50 ~ 80r/min, and the time is 600 ~ 1200min;
4) 3 are tested) viscosity of step ball milling disposed slurry, after ball milling, viscosity controller is at 1000 ~ 6000mPa.s, then slurry is transferred in vacuum defoamation system and carry out deaeration, vacuum degree control-25PSI, stir speed (S.S.) is 30 ~ 120r/min, inclined heated plate 30 ~ 400min, after deaeration, viscosity controller is at 2000 ~ 10000mPa.s;
5) deaeration disposed slurry being pressurized in curtain coating groove, by adjustment curtain coating scraper gap than controlling curtain coating ceramic chips thickness, thus obtaining different thickness casting films;
6) casting films is carried out drying in different warm area, intensification drying rate is controlled by the mode of upper heating, lower heating and wind-heat, warm area arranges drying system: the first warm area temperature is 25 ~ 45 DEG C, second warm area temperature is 40 ~ 60 DEG C, three-temperature-zone temperature is 55 ~ 70 DEG C, four-temperature region temperature is 60 ~ 100 DEG C, and the 5th warm area temperature is 45 ~ 70 DEG C, and the 6th warm area temperature is 25 ~ 50 DEG C; Obtain curtain coating ceramic chips;
7) by cutting inspection, the ceramic chips of desired size is obtained.
2. doctor-blade casting process according to claim 1 is for the preparation of the method for the AlN ceramic chips of multi-layer wire substrate, it is characterized in that:
Described AlN powder requires that mean particle size is between 0.8 ~ 2.5 μm, and specific surface area is 2 ~ 4.5 ㎡/g, and oxygen level is less than 0.9%;
Described sintering aid is rare-earth oxide, alkaline earth metal oxide Y
2o
3, one or both in CaO, MgO;
Described dispersion agent is one or both in oleic acid, triolein, fish oil, acrylic resin;
Described softening agent is one or both in dimethyl phthalate (DMP) and butyl benzyl phthalate (BBP).
3. doctor-blade casting process according to claim 1 is for the preparation of the method for the AlN ceramic chips of multi-layer wire substrate, it is characterized in that:
The mass ratio of described AlN powder, sintering aid, dispersion agent, binding agent, softening agent, solvent can carry out proportioning according to casting thickness.
4. doctor-blade casting process according to claim 1 is for the preparation of the method for the AlN ceramic chips of multi-layer wire substrate, it is characterized in that:
The mass ratio of described AlN powder, sintering aid, dispersion agent, binding agent, softening agent, solvent is 1:0.03 ~ 0.07:0.01 ~ 0.03:0.05 ~ 0.30:0.03 ~ 0.05:0.70 ~ 0.90.
5. the AlN ceramic chips for photoelectric communication industry prepared for the preparation of the method for the AlN ceramic chips of multi-layer wire substrate of a doctor-blade casting process according to claim 1.
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| CN106187201A (en) * | 2015-05-04 | 2016-12-07 | 北京大学 | A kind of flow casting molding without benzene prepares the method for aluminium nitride ceramics |
| CN105130430A (en) * | 2015-08-25 | 2015-12-09 | 深圳百工精艺材料技术有限公司 | Ceramic sheet and preparation method therefor |
| CN109761617B (en) * | 2019-02-22 | 2021-11-05 | 福建臻璟新材料科技有限公司 | F-Ca-Lu doped aluminum nitride complex phase ceramic green body and preparation process thereof |
| CN111592326A (en) * | 2020-06-04 | 2020-08-28 | 黄勇 | High-performance bonding modification excitant for industrial solid waste treatment |
| CN113896540B (en) * | 2021-10-26 | 2022-11-29 | 中国电子科技集团公司第四十三研究所 | Preparation method of aluminum nitride ceramic structural member |
| CN114014669B (en) * | 2021-12-16 | 2023-06-30 | 河北中瓷电子科技股份有限公司 | Preparation method of stretch-proof aluminum nitride raw porcelain substrate |
| CN114890797A (en) * | 2022-04-25 | 2022-08-12 | 中国科学院上海硅酸盐研究所 | Preparation method of silicon nitride ceramic substrate |
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| CN101483417B (en) * | 2009-01-16 | 2011-02-09 | 华中科技大学 | Preparation of black alumina substrate for multilayered wiring |
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